In the current study, an integrated physiochemical method was utilized to remove tonalide (TND) and dimethyl phthalate (DMP) (as emerging contaminants, ECs), and nickel (Ni) and lead (Pb) (as heavy metals), from synthetic wastewater. In the first step of the study, pH, current (mA/cm2), and voltage (V) were set to 7.0, 30, and 9, respectively; then the removal of TND, DMP, Ni, and Pb with an electro-ozonation reactor was optimized using response surface methodology (RSM). At the optimum reaction time (58.1 min), ozone dosage (9.4 mg L−1), initial concentration of ECs (0.98 mg L−1), and initial concentration of heavy metals (28.9 mg L−1), the percentages of TND, DMP, Ni, and Pb removal were 77.0%, 84.5%, 59.2%, and 58.2%, respectively. For the electro-ozonation reactor, the ozone consumption (OC) ranged from 1.1 kg to 3.9 kg (kg O3/kg Ecs), and the specific energy consumption (SEC) was 6.95 (kWh kg−1). After treatment with the optimum electro-ozonation parameters, the synthetic wastewater was transferred to a fixed-bed column, which was filled with a new composite adsorbent (named BBCEC), as the second step of the study. BBCEC improved the efficacy of the removal of TND, DMP, Ni, and Pb to more than 92%.